CN112028637A - Preparation method of high-reliability long-life silicon nitride ceramic ball for aviation bearing - Google Patents
Preparation method of high-reliability long-life silicon nitride ceramic ball for aviation bearing Download PDFInfo
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- CN112028637A CN112028637A CN202010855055.6A CN202010855055A CN112028637A CN 112028637 A CN112028637 A CN 112028637A CN 202010855055 A CN202010855055 A CN 202010855055A CN 112028637 A CN112028637 A CN 112028637A
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 116
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 239000000919 ceramic Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 91
- 238000001694 spray drying Methods 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 34
- 229910052751 metal Inorganic materials 0.000 claims abstract description 28
- 239000002184 metal Substances 0.000 claims abstract description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract description 22
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 230000007062 hydrolysis Effects 0.000 claims abstract description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 110
- 238000000227 grinding Methods 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 26
- 239000011230 binding agent Substances 0.000 claims description 24
- 239000011812 mixed powder Substances 0.000 claims description 22
- 239000002002 slurry Substances 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- 239000003960 organic solvent Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 9
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 claims description 8
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 6
- 235000011285 magnesium acetate Nutrition 0.000 claims description 6
- 239000011654 magnesium acetate Substances 0.000 claims description 6
- 229940069446 magnesium acetate Drugs 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- BYDYILQCRDXHLB-UHFFFAOYSA-N 3,5-dimethylpyridine-2-carbaldehyde Chemical compound CC1=CN=C(C=O)C(C)=C1 BYDYILQCRDXHLB-UHFFFAOYSA-N 0.000 claims description 3
- GAPRPFRDVCCCHR-UHFFFAOYSA-N 3-bromoprop-1-ynyl(trimethyl)silane Chemical compound C[Si](C)(C)C#CCBr GAPRPFRDVCCCHR-UHFFFAOYSA-N 0.000 claims description 3
- JLRJWBUSTKIQQH-UHFFFAOYSA-K lanthanum(3+);triacetate Chemical compound [La+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JLRJWBUSTKIQQH-UHFFFAOYSA-K 0.000 claims description 3
- 239000002243 precursor Substances 0.000 abstract description 8
- 238000005096 rolling process Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 5
- 238000005204 segregation Methods 0.000 abstract description 5
- 150000003839 salts Chemical class 0.000 abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 13
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 10
- 238000004321 preservation Methods 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- 238000005469 granulation Methods 0.000 description 9
- 230000003179 granulation Effects 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 238000009694 cold isostatic pressing Methods 0.000 description 7
- 239000003292 glue Substances 0.000 description 7
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 7
- 238000007599 discharging Methods 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 6
- 239000000395 magnesium oxide Substances 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 238000000498 ball milling Methods 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229920002125 Sokalan® Polymers 0.000 description 3
- 150000001242 acetic acid derivatives Chemical class 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- 239000004584 polyacrylic acid Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000533950 Leucojum Species 0.000 description 1
- 241000519995 Stachys sylvatica Species 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/449—Organic acids, e.g. EDTA, citrate, acetate, oxalate
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Abstract
The invention provides a preparation method of a silicon nitride ceramic ball with high reliability and long service life for an aviation bearing, belonging to the technical field of silicon nitride ceramic ball manufacturing. According to the invention, metal organic salt (aluminum isopropoxide and metal acetate) is used as a precursor of the sintering aid, and the sintering aid can be coated on the surface of silicon nitride through hydrolysis, spray drying and calcination processes, so that the sintering aid is uniformly dispersed in the silicon nitride, and the reduction of the reliability and fatigue life of the ceramic ball caused by agglomeration and segregation of the sintering aid is avoided. The embodiment results show that the compactness of the silicon nitride ceramic ball prepared by the method disclosed by the invention reaches more than 99.9%, the Vickers hardness (HV10) is more than 1500, the crushing load ratio is more than 45%, the Weibull modulus is more than 15, the rolling contact fatigue life (RCF) is more than 400h, and the silicon nitride ceramic ball is particularly suitable for manufacturing rolling elements for aviation bearings.
Description
Technical Field
The invention relates to the technical field of silicon nitride ceramic ball manufacturing, in particular to a preparation method of a silicon nitride ceramic ball with high reliability and long service life for an aviation bearing.
Background
The aviation bearing is one of key core components of an aviation engine, and needs to cope with extremely harsh environments and working conditions such as high speed, high temperature, large maneuverability, large overload, lean lubrication and the like in the aviation field. The performance and quality of the aviation bearing directly influence the service life and reliability of an aviation engine and are one of the main factors influencing the fighting capacity of airplane equipment.
The silicon nitride ceramic has the characteristics of light specific gravity, high rigidity, high temperature resistance, corrosion resistance, wear resistance, self lubrication, electric insulation and the like, has excellent comprehensive performance, and is a preferred material for manufacturing the rolling body for the aviation bearing. At present, a mixed ceramic ball bearing which takes silicon nitride ceramic balls as rolling bodies and takes M50 bearing steel as a ferrule is already used as a main shaft bearing of an aeroengine in the United states. However, the manufacturing technology of the silicon nitride ceramic ball with high reliability and long service life for the domestic aviation bearing is still a 'neck clamping' technology which restricts the development of the aviation engine.
The sintering of the silicon nitride ceramic ball belongs to liquid phase sintering, and a certain amount of sintering aid is required to be added to realize sintering densification. The sintering aid powder and the silicon nitride powder are usually mixed by adopting a mechanical ball milling mode, and although the operation is simple, the uniform mixing of the silicon nitride powder and the sintering aid powder is difficult to realize, so that the agglomeration phenomenon of the sintering aid exists in the mixed powder. The agglomerated sintering aid generates segregation in the sintering process, so that the prepared ceramic ball has the defects of white spots, snowflakes and the like, and the defects can become sources of spalling in the service process of the ceramic ball. Therefore, the agglomeration and segregation of the sintering aid not only reduce the mechanical properties of the silicon nitride ceramic ball, such as strength, hardness and the like, but also seriously affect the reliability and fatigue life of the ceramic ball.
Disclosure of Invention
The invention aims to provide a preparation method of a high-reliability long-life silicon nitride ceramic ball for an aviation bearing, which realizes uniform dispersion of a sintering aid in silicon nitride, and the prepared silicon nitride ceramic ball has high reliability and long fatigue life.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a silicon nitride ceramic ball with high reliability and long service life for an aviation bearing, which comprises the following steps:
mixing aluminum isopropoxide, an organic solvent, silicon nitride powder and a metal acetate aqueous solution, and sequentially performing hydrolysis and first spray drying to obtain mixed powder;
calcining the mixed powder to obtain sintering aid coated silicon nitride powder;
grinding the sintering aid coated silicon nitride powder, mixing the ground silicon nitride powder with a binder, and performing second spray drying to obtain granulated powder;
and sequentially molding, binder removal and sintering the granulated powder to obtain the silicon nitride ceramic ball.
Preferably, the particle diameter D of the silicon nitride powder50alpha-Si of 0.5 to 1.5 μm3N4The content is more than 85 percent, and the oxygen content isThe amount is less than 2%.
Preferably, the metal acetate in the metal acetate aqueous solution comprises one or more of yttrium acetate, magnesium acetate, lanthanum acetate, neodymium acetate and lutetium acetate.
Preferably, the adding amount of the aluminum isopropoxide is 2-8% of the total mass of the sintering aid coated silicon nitride powder based on the amount of the generated aluminum oxide; the adding amount of the metal acetate is 2-8% of the total mass of the sintering aid coated silicon nitride powder by the amount of the generated metal oxide; the adding amount of the silicon nitride powder is 85-95% of the total mass of the sintering aid coated silicon nitride powder.
Preferably, the organic solvent is absolute ethyl alcohol and/or isopropanol.
Preferably, the calcining temperature is 400-600 ℃, and the time is 1-10 h.
Preferably, the solid content of the slurry used in the second spray drying is 40-50%.
Preferably, the particle diameter D of the granulated powder50Is 30 to 150 μm.
Preferably, the temperature of the rubber discharge is 400-600 ℃, and the heat preservation time is 1-10 h.
Preferably, the sintering mode is air pressure sintering, the sintering temperature is 1600-1900 ℃, the heat preservation time is 1-6 h, and the pressure is 0.3-10 MPa.
The invention provides a preparation method of a silicon nitride ceramic ball with high reliability and long service life for an aviation bearing, which comprises the following steps: mixing aluminum isopropoxide, an organic solvent, silicon nitride powder and a metal acetate aqueous solution, and sequentially performing hydrolysis and first spray drying to obtain mixed powder; calcining the mixed powder to obtain sintering aid coated silicon nitride powder; grinding the sintering aid coated silicon nitride powder, mixing the ground silicon nitride powder with a binder, and performing second spray drying to obtain granulated powder; and sequentially molding, binder removal and sintering the granulated powder to obtain the silicon nitride ceramic ball. According to the invention, metal organic salt (aluminum isopropoxide and metal acetate) is used as a precursor of the sintering aid, and the sintering aid can be coated on the surface of silicon nitride through hydrolysis, spray drying and calcination processes, so that the sintering aid is uniformly dispersed in the silicon nitride, and the reduction of the reliability and fatigue life of the ceramic ball caused by agglomeration and segregation of the sintering aid is avoided. The embodiment results show that the compactness of the silicon nitride ceramic ball prepared by the method disclosed by the invention reaches more than 99.9%, the Vickers hardness (HV10) is more than 1500, the crushing load ratio is more than 45%, the Weibull modulus is more than 15, the rolling contact fatigue life (RCF) is more than 400h, and the silicon nitride ceramic ball is particularly suitable for manufacturing rolling elements for aviation bearings.
Detailed Description
The invention provides a preparation method of a silicon nitride ceramic ball with high reliability and long service life for an aviation bearing, which comprises the following steps:
mixing aluminum isopropoxide, an organic solvent, silicon nitride powder and a metal acetate aqueous solution, and sequentially performing hydrolysis and first spray drying to obtain mixed powder;
calcining the mixed powder to obtain sintering aid coated silicon nitride powder;
grinding the sintering aid coated silicon nitride powder, mixing the ground silicon nitride powder with a binder, and performing second spray drying to obtain granulated powder;
and sequentially molding, binder removal and sintering the granulated powder to obtain the silicon nitride ceramic ball.
In the present invention, unless otherwise specified, all the starting materials required for the preparation are commercially available products well known to those skilled in the art.
The method comprises the steps of mixing aluminum isopropoxide, an organic solvent, silicon nitride powder and a metal acetate aqueous solution, and sequentially carrying out hydrolysis and first spray drying to obtain mixed powder. In the present invention, the purity of the aluminum isopropoxide is preferably 99.9% or more. In the invention, the particle diameter D of the silicon nitride powder50Preferably 0.5 to 1.5 μm, alpha-Si3N4The content is > 85%, more preferably > 90%, and the oxygen content is < 2%, more preferably < 1.5%.
In the invention, the metal acetate in the metal acetate aqueous solution preferably comprises one or more of yttrium acetate, magnesium acetate, lanthanum acetate, neodymium acetate and lutetium acetate, and more preferably yttrium acetate or magnesium acetate; when the metal acetates are a plurality of the metal acetates, the proportion of different kinds of metal acetates is not specially limited, and any proportion can be adopted. In the present invention, the purity of the metal acetate is preferably not less than 99.9%. In the invention, the concentration of the metal acetate aqueous solution is preferably 100-500 g/L, and more preferably 200-300 g/L.
In the present invention, the organic solvent is preferably anhydrous ethanol and/or isopropanol; when the organic solvent is preferably absolute ethyl alcohol and isopropanol, the volume ratio of the absolute ethyl alcohol to the isopropanol is not particularly limited in the invention, and any proportion can be used. The amount of the organic solvent used in the present invention is not particularly limited, and the raw materials can be sufficiently dissolved.
In the invention, the addition amount of the aluminum isopropoxide is preferably 2-8% of the total mass of the sintering aid coated silicon nitride powder, and more preferably 3-7% of the total mass of the aluminum oxide; the addition amount of the metal acetate is preferably 2-8% of the total mass of the sintering aid-coated silicon nitride powder, and more preferably 3-7% of the total mass of the generated metal oxide; the adding amount of the silicon nitride powder is preferably 85-95% of the total mass of the sintering aid-coated silicon nitride powder, and more preferably 90%.
In the present invention, the mixing process of the aluminum isopropoxide, the organic solvent, the silicon nitride powder and the metal acetate aqueous solution is preferably that the aluminum isopropoxide is dissolved in the organic solvent, the silicon nitride powder is added to the obtained solution, the stirring is performed for more than 3 hours, so that the silicon nitride powder is dispersed in the organic solvent, then the metal acetate aqueous solution is added, and the stirring is performed for more than 0.5 hours, so as to obtain the mixed solution. And in the stirring process after the metal acetate aqueous solution is added, the aluminum isopropoxide is completely hydrolyzed to form metal hydroxide. The stirring process and the specific time are not particularly limited in the invention, and the materials can be uniformly mixed according to the process well known in the art.
After the mixed liquid is obtained, the mixed liquid is preferably subjected to first spray drying without any residence to obtain mixed powder. In the present invention, the first spray drying mode is preferably nitrogen-protected pressure spray drying or centrifugal spray drying; the present invention does not specifically limit the specific parameters of the first spray drying, and the first spray drying may be performed according to a process well known in the art.
In the invention, the mixed powder is the mixed powder of silicon nitride and a sintering aid precursor. The particle size of the mixed powder is not particularly limited in the present invention, and may be any particle size known in the art.
After the mixed powder is obtained, the mixed powder is calcined to obtain the sintering aid-coated silicon nitride powder. In the invention, the calcining temperature is preferably 400-600 ℃, and the time is preferably 1-10 h. In the calcining process, the precursor of the sintering aid is thermally decomposed to obtain the metal oxide-coated silicon nitride powder, namely the sintering aid-coated silicon nitride powder.
After the sintering aid-coated silicon nitride powder is obtained, the sintering aid-coated silicon nitride powder is ground and then mixed with a binder, and secondary spray drying is carried out to obtain granulation powder. The invention preferably takes absolute ethyl alcohol as solvent and silicon nitride balls as grinding medium balls to grind until the particle diameter D of the powder50Less than or equal to 0.6 mu m to obtain grinding slurry. In the present invention, the apparatus for grinding is preferably a horizontal ball mill, an agitator ball mill or a sand mill. The specification of the grinding medium ball is not specially limited, the specific parameters of grinding are not specially limited, and the powder can reach the particle size range.
After the grinding slurry is obtained, the invention preferably adds the binder into the grinding slurry, stirs for more than 3 hours, and carries out the second spray drying on the obtained mixed material. In the present invention, the binder preferably comprises polyvinyl butyral (PVB) and/or polyacrylic emulsion, and when the binder is PVB and polyacrylic emulsion, the ratio of the PVB to the polyacrylic emulsion is not particularly limited, and can be adjusted according to actual needs; the addition amount of the binder is preferably 0.5-4% of the total mass of the sintering aid-coated silicon nitride powder, and more preferably 1-3%. The stirring process and the specific time are not particularly limited in the present invention, and the raw materials can be uniformly mixed according to the process well known in the art.
In the present invention, the slurry for the second spray drying (i.e., the above-mentioned mixed material) preferably has a solid content of 40 to 50%, more preferably 45%. In the present invention, the second spray drying mode is preferably nitrogen-protected pressure spray drying or centrifugal spray drying; the specific parameters of the second spray drying are not particularly limited in the present invention, and the following particle size of the granulated powder can be achieved by performing the procedures well known in the art.
In the present invention, the particle diameter D of the granulated powder50Preferably 30 to 150 μm, and more preferably 50 to 120 μm.
After the granulation powder is obtained, the invention sequentially carries out molding, binder removal and sintering on the granulation powder to obtain the silicon nitride ceramic ball. In the invention, the forming mode is preferably dry pressing and then cold isostatic pressing, or only cold isostatic pressing is adopted; the invention forms the granulated powder into the ceramic ball by forming.
The dry pressing process is not particularly limited in the present invention, and may be performed according to a process well known in the art. In the invention, the pressure of the cold isostatic pressing is preferably 120-300 MPa, and more preferably 150-250 MPa; other parameters of the cold isostatic pressing are not particularly limited in the present invention and may be performed according to procedures well known in the art.
After the forming is completed, the ceramic ball obtained is preferably subjected to rubber discharge, and the rubber discharge is preferably performed in a flowing air atmosphere or in a vacuum or inert atmosphere. The flow rate of the air atmosphere is not particularly limited in the present invention, and may be performed according to a process well known in the art. In the invention, the temperature of the binder removal is preferably 400-600 ℃, more preferably 450-550 ℃, and the heat preservation time is preferably 1-10 hours, more preferably 2-8 hours. The invention can fully remove the organic matter (binder) in the ceramic ball by removing the glue, thereby reducing the carbon content.
After the binder removal is finished, the ceramic ball is sintered. In the invention, the sintering mode is preferably air pressure sintering, the furnace atmosphere is preferably nitrogen, the sintering temperature is preferably 1600-1900 ℃, more preferably 1700-1800 ℃, the heat preservation time is preferably 1-6 h, more preferably 2-5 h, and the pressure is preferably 0.3-10 MPa. The furnace used for sintering is not particularly limited in the present invention, and a sintering furnace well known in the art may be selected. The invention realizes the densification of the silicon nitride ceramic ball by sintering.
After the sintering is finished, the obtained silicon nitride blank ball is preferably subjected to grinding and polishing in sequence, so that the processing precision of the silicon nitride blank ball reaches the silicon nitride ceramic ball with the grade of G5 or above specified in GBT 308.2-2010. The process of the grinding and polishing process is not particularly limited in the present invention, and the above requirements can be achieved by performing the process according to the well-known art.
According to the invention, the metal organic salt is used as a precursor of the sintering aid, and the sintering aid is coated on the surface of the silicon nitride through hydrolysis, spray drying and calcination, so that the sintering aid is uniformly dispersed in the silicon nitride, and the reduction of the reliability and the fatigue life of the ceramic ball caused by agglomeration and segregation of the sintering aid is avoided.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, the purity of aluminum isopropoxide used was 99.99%, the purity of metal acetate used was 99.99%, and the particle diameter D of silicon nitride powder used was50Is 0.8 mu m, alpha-Si3N4The content is 93 percent, and the oxygen content is 1.2 percent; the spray drying process adopts a nitrogen protection pressure type spray drying mode.
Example 1
12kg (3 kg in terms of alumina) of aluminum isopropoxide (C)9H21AlO3) Dissolving in anhydrous ethanol (100kg), adding 92kg silicon nitride powder, stirring for 3 hr, adding dissolved 15kg (calculated as yttrium oxide amount)5kg) of yttrium acetate (Y (C)2H3O2)3·4H2O) (the concentration of yttrium acetate aqueous solution is 200g/L), stirring for 1.5h, immediately performing spray drying to obtain mixed powder of silicon nitride and sintering aid precursor, and calcining the mixed powder at 450 ℃ for 3h to obtain aluminum oxide and yttrium oxide coated silicon nitride powder (100 kg);
grinding the aluminum oxide and yttrium oxide coated silicon nitride powder in a stirring ball mill for 6 hours by taking absolute ethyl alcohol as a solvent and silicon nitride as a grinding medium ball to ensure that the granularity D of the powder is50The particle size of the slurry is up to below 0.6 micron, 1.5kg of adhesive PVB and 1kg of polyacrylic acid emulsion are added into the ground slurry, the mixture is stirred for 3 hours, the solid content of the slurry is 45%, and granulation powder is obtained after second spray drying is carried out, wherein the particle size D of the granulation powder50About 100 μm;
dry-pressing the granulated powder to form ceramic balls with the diameter of 9.525mm, and then carrying out cold isostatic pressing treatment under the pressure of 250 MPa; carrying out glue discharging on the formed ceramic balls in a flowing air atmosphere, wherein the glue discharging temperature is 450 ℃, and the heat preservation time is 5 h;
sintering the ceramic balls after the binder removal in a gas pressure sintering mode, wherein the sintering temperature is 1800 ℃, the heat preservation time is 2 hours, the atmosphere in a furnace is nitrogen, and the nitrogen pressure is 3MPa, so as to obtain silicon nitride blank balls with the diameter of 9.525 mm;
and sequentially grinding and polishing the silicon nitride blank ball to obtain a G5-grade silicon nitride ceramic fine ball with the processing precision specified in GBT 308.2-2010.
Example 2
20kg (5 kg in terms of alumina) of aluminum isopropoxide (C)9H21AlO3) Dissolving in anhydrous ethanol (120kg), adding 92kg silicon nitride powder, stirring for 3 hr, adding yttrium acetate (Y (C) dissolved with 9kg (3 kg in terms of yttrium oxide) solution2H3O2)3·4H2O) deionized water (the concentration of yttrium acetate aqueous solution is 200g/L), stirring for 2h, immediately spray-drying to obtain mixed powder of silicon nitride and sintering aid precursor, and mixing the mixed powder with the precursorCalcining for 2h at 500 ℃ to obtain aluminum oxide and yttrium oxide coated silicon nitride powder (100 kg);
grinding the aluminum oxide and yttrium oxide coated silicon nitride powder in a stirring ball mill for 6 hours by taking absolute ethyl alcohol as a solvent and silicon nitride as a grinding medium ball to ensure that the granularity D of the powder is50The particle size of the slurry is up to below 0.6 micron, 1.5kg of adhesive PVB and 1kg of polyacrylic acid emulsion are added into the ground slurry, the mixture is stirred for 3 hours, the solid content of the slurry is 45%, and granulation powder is obtained after second spray drying is carried out, wherein the particle size D of the granulation powder50About 100 μm;
dry-pressing the granulated powder to form ceramic balls with the diameter of 9.525mm, and then carrying out cold isostatic pressing treatment under the pressure of 200 MPa; carrying out glue discharging on the formed ceramic balls in a flowing air atmosphere, wherein the glue discharging temperature is 500 ℃, and the heat preservation time is 3 h;
sintering the ceramic balls after the binder removal in a gas pressure sintering mode, wherein the sintering temperature is 1750 ℃, the heat preservation time is 4 hours, the atmosphere in a furnace is nitrogen, and the pressure of the nitrogen is 5MPa, so that silicon nitride blank balls with the diameter of 9.525mm are obtained;
and sequentially grinding and polishing the silicon nitride blank ball to obtain a G5-grade silicon nitride ceramic fine ball with the processing precision specified in GBT 308.2-2010.
Example 3
20kg (5 kg in terms of alumina) of aluminum isopropoxide (C)9H21AlO3) Dissolving in anhydrous ethanol (120L), adding 92kg silicon nitride powder, stirring for 3 hr, adding 16.8kg (3 kg in terms of magnesium oxide) magnesium acetate (Mg (C))2H3O2)2·4H2O) (the concentration of the magnesium acetate aqueous solution is 300g/L), stirring for 2.5h, immediately performing spray drying to obtain mixed powder of silicon nitride and a sintering aid precursor, and calcining the mixed powder at 550 ℃ for 1h to obtain aluminum oxide and magnesium oxide coated silicon nitride powder (100 kg);
grinding the aluminum oxide and magnesium oxide coated silicon nitride powder in a stirring ball mill for 6 hours by taking absolute ethyl alcohol as a solvent and silicon nitride as a grinding medium ball to ensure that the granularity D of the powder is50The particle size of the slurry is up to below 0.6 micron, 1.5kg of adhesive PVB and 1kg of polyacrylic acid emulsion are added into the ground slurry, the mixture is stirred for 3 hours, the solid content of the slurry is 45%, and granulation powder is obtained after second spray drying is carried out, wherein the particle size D of the granulation powder50About 100 μm;
dry-pressing the granulated powder to form ceramic balls with the diameter of 9.525mm, and then carrying out cold isostatic pressing treatment under the pressure of 150 MPa; carrying out glue discharging on the formed ceramic balls in a flowing air atmosphere, wherein the glue discharging temperature is 550 ℃, and the heat preservation time is 2 hours;
sintering the ceramic balls subjected to binder removal in a gas pressure sintering mode, wherein the sintering temperature is 1700 ℃, the heat preservation time is 6 hours, the atmosphere in a furnace is nitrogen, and the nitrogen pressure is 8MPa, so that silicon nitride blank balls with the diameter of 9.525mm are obtained;
and sequentially grinding and polishing the silicon nitride blank ball to obtain a G5-grade silicon nitride ceramic fine ball with the processing precision specified in GBT 308.2-2010.
Comparative example 1
In the comparative example, alumina powder having a purity of 99.99% and a particle diameter D of 99% and yttrium oxide powder as sintering aids were used as the sintering aids in the same amounts as in example 1500.5 μm, the purity of the yttrium oxide powder is 99.99%, and the particle diameter D500.8 μm; mixing and grinding the sintering aid powder and the silicon nitride powder in a mechanical ball milling mode for 6 hours, and testing the particle size D of the powder50After reaching the same level (below 0.6 μm) as in example 1, a binder was added to the slurry obtained by grinding (same as in example 1), stirred for 3 hours, and spray-dried to obtain granulated powder, and the other process conditions were the same as in example 1.
Comparative example 2
In the comparative example, alumina powder and yttrium oxide powder were directly used as sintering aids, the addition amount of the sintering aids was the same as that of the sintering aid in example 2, the purity of the alumina powder was 99.99%, and the particle size D was the same as that of the alumina powder50Is 0.5 micron, the purity of the yttrium oxide powder is 99.99 percent, and the particle size D50Is 0.8 microns. The sintering is carried out by adopting a mechanical ball milling modeMixing and grinding the bonding assistant powder and the silicon nitride powder, wherein the mixing and grinding time is 6h, and the particle diameter D of the tested powder50After reaching the same level (less than 0.6 micron) as in example 2, the binder was added to the slurry obtained by grinding (same as in example 2), stirred for 3 hours or more, and spray-dried to obtain granulated powder, and the other process conditions were the same as those in example 2.
Comparative example 3
In the comparative example, alumina powder and magnesia powder are used as sintering aids, and the addition amount of the sintering aids is the same as that of the sintering aids in example 3; the purity of the alumina powder is 99.99 percent, and the grain diameter D is50Is 0.5 micron, the purity of the magnesium oxide powder is 99.9 percent, and the particle diameter D500.5 micron; mixing and grinding the sintering aid powder and the silicon nitride powder in a mechanical ball milling mode for 6 hours, and testing the particle size D of the powder50After reaching the same level (less than 0.6 micron) as in example 3, the binder was added to the slurry obtained by grinding (same as in example 3), stirred for 3 hours or more, and spray-dried to obtain granulated powder, and the other process conditions were the same as those in example 3.
Performance testing
The densities of the silicon nitride ceramic balls in examples 1 to 3 and comparative examples 1 to 3 were measured by the archimedes drainage method, and the relative densities thereof were calculated. The vickers hardness (HV10) of the ceramic balls was measured using the method specified in GBT 16534-. The crushing load of the ceramic balls was measured according to the three-ball test method specified in the JB/T1255-2001 standard, and the crushing load ratio (the ratio of the crushing load that the ceramic balls can bear to the crushing load that the steel balls of the same specification can bear) was calculated. And testing 30 groups of crushing load data in each case, fitting the 30 groups of crushing load data to obtain a Weibull modulus, and taking the Weibull modulus as an evaluation basis of the reliability of the ceramic ball. The rolling contact fatigue life of the ceramic balls was tested using the method described in patent CN102951905A (maximum contact stress of 5.9GPa, rotation speed of 1200 rpm). Table 1 shows the measured data.
TABLE 1 Performance data for silicon nitride ceramic balls prepared in examples 1-3 and comparative examples 1-3
As can be seen from Table 1, under the same other process conditions, the density of the ceramic ball prepared by coating silicon nitride with the sintering aid reaches over 99.9 percent, the Vickers hardness (HV10) is over 1500, the crushing load ratio is over 45 percent, the Weibull modulus is over 15, and the rolling contact fatigue life is over 400 hours. In contrast, the ceramic ball prepared by coating the silicon nitride with the sintering aid has better performance than the ceramic ball prepared by directly adding the sintering aid powder, and particularly, the reliability and the fatigue life are greatly improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a silicon nitride ceramic ball with high reliability and long service life for an aviation bearing comprises the following steps:
mixing aluminum isopropoxide, an organic solvent, silicon nitride powder and a metal acetate aqueous solution, and sequentially performing hydrolysis and first spray drying to obtain mixed powder;
calcining the mixed powder to obtain sintering aid coated silicon nitride powder;
grinding the sintering aid coated silicon nitride powder, mixing the ground silicon nitride powder with a binder, and performing second spray drying to obtain granulated powder;
and sequentially molding, binder removal and sintering the granulated powder to obtain the silicon nitride ceramic ball.
2. The preparation method according to claim 1, wherein the particle diameter D of the silicon nitride powder50alpha-Si of 0.5 to 1.5 μm3N4The content is more than 85 percent, and the oxygen content is less than 2 percent.
3. The method according to claim 1, wherein the metal acetate in the aqueous solution of metal acetate comprises one or more of yttrium acetate, magnesium acetate, lanthanum acetate, neodymium acetate, and lutetium acetate.
4. The preparation method according to claim 1, wherein the aluminum isopropoxide is added in an amount of 2-8% of the total mass of the sintering aid coated silicon nitride powder, based on the amount of aluminum oxide generated; the adding amount of the metal acetate is 2-8% of the total mass of the sintering aid coated silicon nitride powder by the amount of the generated metal oxide; the adding amount of the silicon nitride powder is 85-95% of the total mass of the sintering aid coated silicon nitride powder.
5. The method according to claim 1, wherein the organic solvent is absolute ethanol and/or isopropanol.
6. The preparation method according to claim 1, wherein the calcination is carried out at a temperature of 400 to 600 ℃ for 1 to 10 hours.
7. The method according to claim 1, wherein the slurry for the second spray drying has a solid content of 40 to 50%.
8. The method according to claim 1, wherein the granulated powder has a particle diameter D50Is 30 to 150 μm.
9. The preparation method according to claim 1, wherein the temperature of the binder removal is 400-600 ℃, and the holding time is 1-10 h.
10. The preparation method according to claim 1, wherein the sintering mode is air pressure sintering, the sintering temperature is 1600-1900 ℃, the holding time is 1-6 h, and the pressure is 0.3-10 MPa.
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